CN111348913A - High bandwidth piezoelectric ceramic and preparation method thereof - Google Patents
High bandwidth piezoelectric ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-bandwidth piezoelectric ceramic and a preparation method thereof, belonging to the preparation method of electronic components; aims to provide a piezoelectric ceramic which can widen the application range and has the structural general formula as follows: (0.98-x) Pb (Zr, Ti) O3‑xBiFeO3‑0.02Pb(Sb1/ 3Nb2/3)O3+yat%SrCO3+zat%BaCO3(ii) a Wherein Zr/Ti = 1.35-1.2, x = 0.01-0.05, y = 0.05-0.1, and z = 0.07-0.1; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 90-98.5 wt%. The preparation method of the piezoelectric ceramic comprises the following steps: proportioning, ball milling, presintering, secondary ball milling, molding, binder removal, sintering, silver electrode coating and polarization; the piezoelectric ceramic of the present invention has excellent dielectric and piezoelectric properties, d33≥750pC/N、ε33 T/ε0Not less than 3800, and not less than 30% bandwidth △ f, and can be widely used in buzzer, alarm, and piezoelectric pump.
Description
Technical Field
The invention relates to a piezoelectric ceramic and a preparation method thereof, in particular to a high-bandwidth piezoelectric ceramic and a preparation method thereof; belongs to a preparation method of electronic components.
Background
The piezoelectric buzzer, the alarm and the piezoelectric pump realize sound production or liquid transmission by utilizing the inverse piezoelectric effect of the piezoelectric ceramic piece to generate mechanical deformation; the device has the advantages of high reliability, low power consumption, low noise, small volume and the like.
The bandwidth of the piezoceramic wafer determines to a large extent the sound pressure of the sound-generating device. Generally, when the bandwidth is more than or equal to 18%, the sound pressure of the corresponding generating device is more than or equal to 80db, and the use requirement can be met; but the use requirements cannot be met in outdoor or noisy environment, so that the use range of the buzzer and the alarm is limited.
The bandwidth of the piezoceramic wafer determines the flow rate of the piezoelectric pump. Generally, when the bandwidth is more than or equal to 20%, the flow rate of the piezoelectric pump is more than or equal to 300mL/min, and the requirement of the fish culture oxygenation pump can be met; but cannot meet the requirements of devices with higher flow, such as a water dispenser, an aromatherapy machine, a humidifier and the like.
Therefore, in order to widen the application range of the sound generating device or the piezoelectric pump, it is necessary to increase the bandwidth of the piezoelectric ceramic plate.
Disclosure of Invention
Aiming at the defect that the citation range of the piezoelectric ceramic piece is limited due to the fact that the bandwidth of the piezoelectric ceramic piece is narrow in the prior art, the invention aims to provide the high-bandwidth piezoelectric ceramic and the preparation method thereof.
In order to achieve the above object, the general structural formula of the high-bandwidth piezoelectric ceramic provided by the invention is as follows:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3(ii) a Wherein Zr/Ti = 1.35-1.2, x = 0.01-0.05, y = 0.05-0.1, and z = 0.07-0.1; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 90-98.5 wt%.
Preferably, Zr/Ti = 1.3-1.25;
preferably, x = 0.03;
preferably, y = 0.08;
preferably, z = 0.085.
In order to prepare the high-bandwidth piezoelectric ceramic, the preparation method adopts the following technical scheme:
1) mixing and ball milling Pb3O4、ZrO2、TiO2、Nb2O5、Fe2O3、Sb2O3、Bi2O3、SrCO3、BaCO3Proportioning according to the stoichiometric ratio of the structural general formula, ball-milling for 4h, drying, and sieving with a 40-mesh sieve to obtain mixed powder; zirconia balls are prepared from deionized water =2:1: 1;
2) pre-sintering, heating the mixed powder to 900 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 2 hours to cool along with the furnace to obtain clinker;
3) performing secondary ball milling to ball mill the clinker for 4 hours, drying and sieving by a 40-mesh sieve to obtain cooked powder; zirconia balls are prepared from deionized water =2:1: 0.8;
4) molding, namely adding 20wt% of PVA into the cooked powder, uniformly mixing, and then performing die binding molding to obtain a porcelain blank;
5) the ceramic blank is sent into a sintering furnace to be heated to 600 ℃ at the speed of 0.5 ℃/min for binder removal and sintering, and then is heated to 1270 ℃ at the speed of 1.5 ℃/min for sintering, and the ceramic blank is cooled along with the furnace after being kept warm for 3 hours to obtain a ceramic wafer;
6) printing silver paste on the surface of the ceramic chip by a silver electrode, drying, and then burning silver for 2 hours in a tunnel furnace at 780 ℃ to obtain a ceramic chip of the silver electrode;
7) and (3) polarizing the silver electrode ceramic wafer for 30min at the temperature of 100 ℃ and under the voltage of 1.4KV/mm, and standing for 24 h.
Compared with the prior art, the piezoelectric ceramic prepared by the formula and the preparation method provided by the invention has excellent dielectric and piezoelectric properties, and d33≥750pC/N、ε33 T/ε0The piezoelectric pump has the advantages of being more than or equal to 3800, having the bandwidth △ f more than or equal to 30%, being widely applied to buzzers, alarms and piezoelectric pumps, having simple preparation process and low cost, and being easy for batch production.
Detailed Description
The invention is further illustrated by the following specific examples:
example 1 preparation of a compound of the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.35, x =0.01, y =0.05, z = 0.07; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 98.5 wt%; the method comprises the following steps:
1) the mixture is ball milled at room temperature and in the environment with relative air humidity more than or equal to 60 percent, and Pb with purity more than or equal to 99 percent is obtained3O4、ZrO2、TiO2、Nb2O5、Fe2O3、Sb2O3、Bi2O3、SrCO3、BaCO3Proportioning according to the stoichiometric ratio of the structural general formula, adding zirconia balls, the raw materials and deionized water into a planetary ball mill according to the weight ratio of 2:1:1, ball-milling for 4 hours, drying, and sieving with a 40-mesh sieve to obtain mixed powder;
2) pre-sintering, namely pressing the mixed powder under the pressure of 20Mpa into blocks of phi 50 × 5 mm, feeding the blocks into a box-type furnace, heating to 900 ℃ at the speed of 2.5 ℃/min, preserving heat for 2h, cooling along with the furnace, and crushing to obtain clinker;
3) adding zirconia balls, the clinker and deionized water into a planetary ball mill according to the weight ratio of 2:1:0.8 for ball milling for 4 hours, drying and sieving by a 40-mesh sieve to obtain cooked powder;
4) molding, adding 20wt% of PVA into the cooked powder, uniformly mixing, and then rolling into a ceramic blank with the diameter of phi 36 × 0.3 mm of 0.3 mm;
5) the ceramic blank is sent into a box type furnace to be heated to 600 ℃ at the speed of 0.5 ℃/min for binder removal and sintering, and then is heated to 1270 ℃ at the speed of 1.5 ℃/min for sintering, and the ceramic blank is cooled along with the furnace after being kept warm for 3 hours to obtain a ceramic plate;
6) printing silver paste on the surface of the ceramic chip by a silver electrode, drying in a tunnel furnace, and then burning silver for 2h in an environment of 780 ℃ to obtain a ceramic chip of the silver electrode;
7) and (3) polarizing the silver electrode ceramic wafer for 30min at the voltage of 1.4KV/mm in the environment of 100 ℃, and standing for 24 h.
The bandwidth (△ f) of the piezoelectric ceramic prepared in this example was directly measured on an impedance analyzer according to the formula △ f = (f)p/fs-1) × 100% by 100%, wherein fpIs anti-resonance frequency (KHz), fsAt resonant frequency (KHz); the test results are shown in Table 1.
Example 2 the general structural formula was prepared as in example 1:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.35, x =0.03, y =0.08, z = 0.085; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 96.7 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 3 the general structural formula was prepared as in example 1:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.35, x =0.05, y =0.1, z = 0.1; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 90.1 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 4 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.3, x =0.01, y =0.05, z = 0.07; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 98.2 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 5 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.3, x =0.03, y =0.08, z = 0.085; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 95.9 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 6 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.3, x =0.05, y =0.1, z = 0.1; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 91.4 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 7 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.25, x =0.01, y =0.05, z = 0.07; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 98 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 8 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.25, x =0.03, y =0.08, z = 0.085; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 95.3 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 9 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.25, x =0.05, y =0.1, z = 0.1; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 91.8 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 10 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.2, x =0.01, y =0.05, z = 0.07; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 97.6 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 11 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.2, x =0.03, y =0.08, z = 0.085; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 94.9 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Example 12 the general structural formula:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3
the high bandwidth piezoelectric ceramic of (1); wherein Zr/Ti =1.2, x =0.05, y =0.1, z = 0.1; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 92.3 wt%; the bandwidth of the piezoelectric ceramic prepared in this example was measured by the method of example 1, and the measurement results are shown in table 1.
Table 1: the invention relates to a test meter for electrical performance indexes of piezoelectric ceramics
The following are a set of general structural formulas prepared according to the method of example 1: (0.98-x) Pb (Zr, Ti) O3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3And the bandwidth of each comparative piezoelectric ceramic was measured in the same manner as in example 1.
Comparative example 1 wherein Zr/Ti =1.35, y =0.05, z =0.07, the proportion of niobium antimony-lead zirconate titanate ternary system in the structural formula is 98.4 wt%; the test results are shown in Table 2.
Comparative example 2 wherein Zr/Ti =1.35, y =0.1, z =0.1, and the proportion of the niobium antimony-lead zirconate titanate ternary system in the structural formula is 90.5 wt%; the test results are shown in Table 2.
Comparative example 3, wherein Zr/Ti =1.3, y =0.05, z =0.07, the proportion of niobium antimony-lead zirconate titanate ternary system in the structural general formula is 98.2 wt%; the test results are shown in Table 2.
Comparative example 4, wherein Zr/Ti =1.3, y =0.1, z =0.1, and the proportion of the niobium antimony-lead zirconate titanate ternary system in the structural general formula is 90.3 wt%; the test results are shown in Table 2.
Comparative example 5, wherein Zr/Ti =1.25, y =0.05, z =0.07, the proportion of niobium antimony-lead zirconate titanate ternary system in the structural general formula is 98 wt%; the test results are shown in Table 2.
Comparative example 6 wherein Zr/Ti =1.25, y =0.1, z =0.1, and the proportion of the niobium antimony-lead zirconate titanate ternary system in the general structural formula is 90.2 wt%; the test results are shown in Table 2.
Comparative example 7, wherein Zr/Ti =1.2, y =0.05, and z =0.07, the proportion of the niobium antimony-lead zirconate titanate ternary system in the structural formula is 97.9 wt%; the test results are shown in Table 2.
Comparative example 8, wherein Zr/Ti =1.2, y =0.1, z =0.1, and the proportion of the niobium antimony-lead zirconate titanate ternary system in the structural general formula is 90 wt%; the test results are shown in Table 2.
In the above comparative examples, the purity of each raw material was not less than 99%.
Table 2: the piezoelectric ceramic prepared by the method of the invention has the electrical performance index test meter
| Parameter(s) | Relative dielectric constant ε33 T/ε0 | Piezoelectric constant (pC/N) | Bandwidth (△ f) |
| Comparative example 1 | 3845 | 719 | 18% |
| Comparative example 2 | 4156 | 741 | 20% |
| Comparative example 3 | 3844 | 725 | 19% |
| Comparative example 4 | 4221 | 790 | 22% |
| Comparative example 5 | 4115 | 811 | 22% |
| Comparative example 6 | 4325 | 801 | 21% |
| Comparative example 7 | 3836 | 756 | 19% |
| Comparative example 8 | 3996 | 783 | 19% |
As can be seen from tables 1 and 2, the piezoelectric constant d of the piezoelectric ceramic sheet prepared by the formula and the method of the invention33Not less than 750 (pC/N), relative dielectric constant epsilon33 T/ε03800, △ f and 27 f, excellent piezoelectric and dielectric performance, great bandwidth, and wide application in buzzer, alarm and piezoelectric pump.
Claims (6)
1. A high bandwidth piezoelectric ceramic is characterized in that the structural general formula is as follows:
(0.98-x)Pb(Zr,Ti)O3-xBiFeO3-0.02Pb(Sb1/3Nb2/3)O3+yat%SrCO3+zat%BaCO3(ii) a Wherein Zr/Ti = 1.35-1.2, x = 0.01-0.05, y = 0.05-0.1, and z = 0.07-0.1; the proportion of the niobium antimony-bismuth ferrite-lead zirconate titanate quaternary system in the structural general formula is 90-98.5 wt%.
2. The high bandwidth piezoelectric ceramic of claim 1, wherein: Zr/Ti = 1.3-1.25.
3. The high-bandwidth piezoelectric ceramic according to claim 1 or 2, wherein: x = 0.03.
4. The high-bandwidth piezoelectric ceramic according to claim 1 or 2, wherein: y = 0.08.
5. The high-bandwidth piezoelectric ceramic according to claim 1 or 2, wherein: z = 0.085.
6. A method for preparing a high bandwidth piezoelectric ceramic according to any one of claims 1 to 5, characterized by the steps of:
1) mixing and ball milling Pb3O4、ZrO2、TiO2、Nb2O5、Fe2O3、Sb2O3、Bi2O3、SrCO3、BaCO3Proportioning according to the stoichiometric ratio of the structural general formula, ball-milling for 4h, drying, and sieving with a 40-mesh sieve to obtain mixed powder; zirconia balls are prepared from deionized water =2:1: 1;
2) pre-sintering, heating the mixed powder to 900 ℃ at the speed of 2.5 ℃/min, and keeping the temperature for 2 hours to cool along with the furnace to obtain clinker;
3) performing secondary ball milling to ball mill the clinker for 4 hours, drying and sieving by a 40-mesh sieve to obtain cooked powder; zirconia balls are prepared from deionized water =2:1: 0.8;
4) molding, namely adding 20wt% of PVA into the cooked powder, uniformly mixing, and then performing die binding molding to obtain a porcelain blank;
5) the ceramic blank is sent into a sintering furnace to be heated to 600 ℃ at the speed of 0.5 ℃/min for binder removal and sintering, and then is heated to 1270 ℃ at the speed of 1.5 ℃/min for sintering, and the ceramic blank is cooled along with the furnace after being kept warm for 3 hours to obtain a ceramic wafer;
6) printing silver paste on the surface of the ceramic chip by the silver electrode, drying, and then burning silver for 2h in an environment of 780 ℃ to obtain a ceramic chip of the silver electrode;
7) and (3) polarizing the silver electrode ceramic wafer for 30min at the temperature of 100 ℃ and under the voltage of 1.4KV/mm, and standing for 24 h.
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